Chemical synthesis of nanocrystalline CuAlO2 via nitrate-citrate combustion route

The nanocrystalline delafossite CuAlO2 powder was synthesised by a sol-gel nitrate-citrate self-combustion route. Citric acid was introduced both as the chelating and reducing agent or fuel. The citric acid/metal ion ratio was adjusted to provide fuel-lean, stoichiometric or fuel-rich conditions of the redox reaction. Equimolar amounts of copper and aluminium nitrates and the citric acid were dissolved in deionized water. The sol was dried at 80 oC to obtain the gel. By increasing the temperature above 250 oC, the gel immediately ignited, forming the precursor powder. According to the X-ray diffraction analysis the phase pure delafossite was obtained only when the precursor powder was prepared from the stoichiometric redox reaction, and after the calcination for 4 h in Ar atmosphere at 920 oC. The field emission scanning electron micrographs revealed the cauliflower aspect of the calcined powder, where small primary particles formed the agglomerates. The formation of the phase pure CuAlO2 powder was also confirmed by Fourier transformed infrared spectroscopy

Screen Printed Copper and Tantalum Modified Potassium Sodium Niobate Thick Films on Platinized Alumina Substrates

We show how sintering in different atmospheres affects the structural, microstructural, and functional properties of ~30 μm thick films of K0.5Na0.5NbO3 (KNN) modified with 0.38 mol% K5.4Cu1.3Ta10O29 and 1 mol% CuO. The films were screen printed on platinized alumina substrates and sintered at 1100 °C in oxygen or in air with or without the packing powder (PP). The films have a preferential crystallographic orientation of the monoclinic perovskite phase in the [100] and [−101] directions. Sintering in the presence of PP contributes to obtaining phase-pure films, which is not the case for the films sintered without any PP notwithstanding the sintering atmosphere. The latter group is characterized by a slightly finer grain size, from 0.1 μm to ~2 μm, and lower porosity, ~6% compared with ~13%. Using piezoresponse force microscopy (PFM) and electron backscatter diffraction (EBSD) analysis of oxygen-sintered films, we found that the perovskite grains are composed of multiple domains which are preferentially oriented. Thick films sintered in oxygen exhibit a piezoelectric d33 coefficient of 64 pm/V and an effective thickness coupling coefficient kt of 43%, as well as very low mechanical losses of less than 0.5%, making them promising candidates for lead-free piezoelectric energy harvesting applications

Lead-Free Sodium Potassium Niobate-Based Multilayer Structures for Ultrasound Transducer Applications

Thick films with nominal composition (K0.5Na0.5)0.99Sr0.005NbO3 (KNNSr) on porous ceramics with identical nominal composition were investigated as potential candidates for environmentally benign ultrasonic transducers composed entirely of inorganic materials. In this paper, the processing of the multilayer structure, namely, the thick film by screen printing and the porous ceramic by sacrificial template method, is related to their phase composition, microstructure, electromechanical, and acoustic properties to understand the performance of the devices. The ceramic with a homogeneous distribution of 8 μm pores had a sufficiently high attenuation coefficient of 0.5 dB/mm/MHz and served as an effective backing. The KNNSr thick films sintered at 1100 °C exhibited a homogeneous microstructure and a relative density of 97%, contributing to a large dielectric permittivity and elastic constant and yielding a thickness coupling factor kt of ~30%. The electroacoustic response of the multilayer structure in water provides a centre frequency of 15 MHz and a very large fractional bandwidth (BW) of 127% at −6 dB. The multilayer structure is a candidate for imaging applications operating above 15 MHz, especially by realising focused-beam structure through lenses to further increase the sensitivity in the focal zone

Chemical Solution Deposition of Barium Titanate Thin Films with Ethylene Glycol as Solvent for Barium Acetate

Chemical solution deposition (CSD) of BaTiO3 (BT) or BT-based thin films relies on using a carboxylic acid and alcohol as the solvents for alkaline-earth carboxylate and transition-metal alkoxide, respectively; however, the esterification reaction of the solvents may lead to in-situ water formation and precipitation. To avoid such an uncontrolled reaction, we developed a route in which ethylene glycol (EG) is used as the solvent for Ba-acetate. The EG-based BT coating solutions are stable for at least a few months. The thermal decomposition of the BT xerogel obtained by drying the EG-based solutions depends on the choice of the solvent for the Ti-alkoxide as well: in the case of EG and 2-methoxyethanol solvents carbon residues are removed at only about 1100 °C, while in the case of ethanol it is concluded at about 700 °C. About 100 nm thick BT films derived from the EG-ethanol solution deposited on platinized silicon reveal dense, crack-free columnar microstructure. They exhibit local ferro- and piezoelectric properties. The macroscopic polarization-electric field loops were obtained up to a quite high electric field of about 2.4 MV/cm. The EG-ethanol based CSD route is a viable alternative to the established acetic acid–alcohol route for BT and BT-based films

Indium-zinc-oxide thin films produced by low-cost chemical solution deposition: Tuning the microstructure, optical and electrical properties with the processing conditions

Indium-zinc-oxide (IZO) films were prepared by spin coating an ethanol-ethylene-glycol precursor solution with a Zn/(In + Zn) ratio of 0.36 on glass. The effects of temperature on the structure, microstructure, electrical, and optical properties of the IZO thin films were investigated by thermal analysis, Fourier-transform infrared spectroscopy, X-ray diffraction, electron and atomic-force microscopy, X-ray photoelectron spectroscopy and variable-angle spectroscopic ellipsometry. The prepared IZO thin films heated at 500, 600, and 700 °C in air were transparent, without long-range ordering, and with an RMS surface roughness of less than 1 nm. The lowest electrical resistivity at room temperature, 0.0069 Ωcm, was observed for the 115-nm-thick IZO thin film heated at 600 °C in air and subsequently post-annealed in Ar/H2. The thin film exhibited a microstructure characterized by grains typically 20 nm in size and had no organic residues. This film exhibits uniaxial optical anisotropy due to its ultra-thin lamellae with a high electron density. The ordinary refractive index was fitted as a Tauc-Lorentz-Urbach function, which is typical of an indirect absorption edge occurring in amorphous semiconductor materials. The principal absorption peak with an onset at about 2.8 eV and a Tauc gap energy of ∼2.6 eV is similar to those observed for In2O3. The described process of chemical solution deposition and subsequent curing is promising for the low-cost fabrication of IZO thin films for transparent electronics, and can be used to tune the structure and microstructure of IZO thin films, as well as their electrical and optical properties

Crystallization of piezoceramic films on glass via flash lamp annealing

Abstract Integration of thin-film oxide piezoelectrics on glass is imperative for the next generation of transparent electronics to attain sensing and actuating functions. However, their crystallization temperature (above 650 °C) is incompatible with most glasses. We developed a flash lamp process for the growth of piezoelectric lead zirconate titanate films. The process enables crystallization on various types of glasses in a few seconds only. The functional properties of these films are comparable to the films processed with standard rapid thermal annealing at 700 °C. A surface haptic device was fabricated with a 1 μm-thick film (piezoelectric e 33,f of −5 C m−2). Its ultrasonic surface deflection reached 1.5 μm at 60 V, sufficient for its use in surface rendering applications. This flash lamp annealing process is compatible with large glass sheets and roll-to-roll processing and has the potential to significantly expand the applications of piezoelectric devices on glass

Screen printed copper and tantalum modified potassium sodium niobate thick films on platinized alumina substrates

We show how sintering in different atmospheres affects the structural, microstructural, and functional properties of ~30 μm thick films of K0.5Na0.5NbO3 (KNN) modified with 0.38 mol% K5.4Cu1.3Ta10O29 and 1 mol% CuO. The films were screen printed on platinized alumina substrates and sintered at 1100 °C in oxygen or in air with or without the packing powder (PP). The films have a preferential crystallographic orientation of the monoclinic perovskite phase in the [100] and [−101] directions. Sintering in the presence of PP contributes to obtaining phase-pure films, which is not the case for the films sintered without any PP notwithstanding the sintering atmosphere. The latter group is characterized by a slightly finer grain size, from 0.1 μm to ~2 μm, and lower porosity, ~6% compared with ~13%. Using piezoresponse force microscopy (PFM) and electron backscatter diffraction (EBSD) analysis of oxygen-sintered films, we found that the perovskite grains are composed of multiple domains which are preferentially oriented. Thick films sintered in oxygen exhibit a piezoelectric d33 coefficient of 64 pm/V and an effective thickness coupling coefficient kt of 43%, as well as very low mechanical losses of less than 0.5%, making them promising candidates for lead-free piezoelectric energy harvesting applications

Fermi energy, electrical conductivity, and the energy gap of NaNbO 3

The energy of the valence band maximum of NaNbO3 is determined from the Schottky barrier heights at the contacts with low work function Sn-doped In 2 O3 and high work function RuO2 by means of x-ray photoelectron spectroscopy with in situ interface preparation. The measurements reveal a valence-band edge energy, which is comparable to that of SrTiO3 and BaTiO3 . The energy gap of SrTiO3 and BaTiO3 is 3.2 eV and comparable to the values of 3.4 eV to 3.5 eV, which are determined by means of optical and electron energy loss spectroscopy for NaNbO 3 . It is therefore expected that the conduction band minimum of NaNbO3 is also located at a similar energy as the conduction band minimum of SrTiO3 and BaTiO3 . If this is the case, it can be expected that donor doping of NaNbO3 leads to an electrical conductivity, which is comparable to those of donor-doped SrTiO3 and BaTiO3 (up to ∼ 1 S/cm−1 ). In contrast, Sr- and Ca-doped NaNbO3 bulk ceramics exhibit a room temperature conductivity up to 10 × 10−10 S/cm−1 , only slightly higher than that of NaNbO 3 . High-field conductivity measurements and impedance spectroscopy give no indication that the low conductivity is caused by insulating grain boundaries separating electrically conductive grains. It is therefore suggested that the energy gap of NaNbO 3 is substantially higher than the gap of 3.4 eV to 3.5 eV determined from optical spectroscopy reported in literature and from electron energy loss spectroscopy within this paper, as also suggested from electronic structure calculations of LiNbO3